#------------------------------------------------------------------------------
#$Date: 2024-05-05 05:50:17 +0300 (Sun, 05 May 2024) $
#$Revision: 291625 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/55/7715593.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715593
loop_
_publ_author_name
'Mączka, Mirosław'
'Sobczak, Szymon'
'Ptak, Maciej'
'Smółka, Szymon'
'Fedoruk, Katarzyna'
'Dybała, Filip'
'Herman, Artur P.'
'Paraguassu, Waldeci'
'Zaręba, Jan K'
'Kudrawiec, Robert'
'Sieradzki, Adam'
'Katrusiak, Andrzej'
_publ_section_title
;
 Revisiting a (001)-oriented layered lead chloride templated by
 1,2,4-triazolium: structural phase transitions, lattice dynamics and
 broadband photoluminescence.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6906
_journal_page_last               6919
_journal_paper_doi               10.1039/d4dt00406j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_name_systematic        Tz2PbCl4
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2959(15)
_cell_length_b                   7.4918(15)
_cell_length_c                   21.829(6)
_cell_measurement_reflns_used    2933
_cell_measurement_temperature    340.00(10)
_cell_measurement_theta_max      28.7340
_cell_measurement_theta_min      2.7760
_cell_volume                     1356.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      340.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7067
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.889
_diffrn_reflns_theta_min         3.782
_exptl_absorpt_coefficient_mu    13.203
_exptl_absorpt_correction_T_max  0.255
_exptl_absorpt_correction_T_min  0.059
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.395
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.929
_refine_diff_density_min         -2.164
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0415P)²+9.5938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                765
_reflns_number_total             905
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00406j2.cif
_cod_data_source_block           triag2pbcl4_340a
_cod_depositor_comments
'Adding full bibliography for 7715584--7715597.cif.'
_cod_database_code               7715593
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.300
_shelx_estimated_absorpt_t_min   0.051
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Shared sites
{C2, N2}
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(N2)
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C2(0.5) H2(0.5) N2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1A), N1(H1B), C2(H2), C1(H1)
;
_shelx_res_file
;
TITL triag2pbcl4_340a_a.res in Cmcm
    triag2pbcl4_340a.res
    created by SHELXL-2018/3 at 13:08:43 on 15-Dec-2023
REM Old TITL TRIAG2PbCl4_340a in Cmcm
REM SHELXT solution in Cmcm: R1 0.107, Rweak 0.034, Alpha 0.009
REM <I/s> 2.044 for 63 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 N4 Cl4 Pb
CELL 0.71073 8.2959 7.4918 21.8291 90 90 90
ZERR 4 0.0015 0.0015 0.0058 0 0 0
LATT 7
SYMM -X,-Y,0.5+Z
SYMM -X,+Y,0.5-Z
SYMM +X,-Y,-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
EADP C2 N2
EXYZ C2 N2

L.S. 44
PLAN  1
SIZE 0.12 0.18 0.56
TEMP 67
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT 0 0 4
OMIT 0 0 6
OMIT 0 10 1
OMIT 1 1 0
OMIT 1 1 4
OMIT 2 0 0
OMIT 2 2 0
OMIT 3 1 1
OMIT 4 0 0
OMIT 4 0 2
OMIT 5 1 1
OMIT 6 2 0
OMIT 7 7 8
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_340a.hkl">
REM </olex2.extras>

WGHT    0.041500    9.593801
SWAT    0.217481    0.1793
FVAR       2.86304
PB1   5    0.500000    0.244898    0.250000    10.25000    0.01946    0.02413 =
         0.03487    0.00000    0.00000    0.00000
CL2   3    0.500000    0.244711    0.118611    10.50000    0.03438    0.12389 =
         0.03895    0.00051    0.00000    0.00000
CL1   3    0.749580    0.494604    0.250000    10.50000    0.07335    0.07471 =
         0.10730    0.00000    0.00000   -0.05363
N1    4    0.124088    0.244426    0.101673    11.00000    0.03454    0.11249 =
         0.08229    0.00376   -0.01335   -0.00446
PART 11
AFIX  43
H1A   2    0.222530    0.246236    0.114005    10.50000   -1.20000
AFIX  43
PART 12
H1B   2    0.222530    0.246236    0.114005    10.50000   -1.20000
AFIX   0
PART 11
C2    1    0.079955    0.242691    0.044451    10.50000    0.08333    0.29000 =
         0.05261   -0.00544    0.02262    0.00049
AFIX  43
H2    2    0.147158    0.241656    0.010353    10.50000   -1.20000
AFIX   0
PART 0
C1    1    0.000000    0.243062    0.137432    10.50000    0.06647    0.08984 =
         0.05241    0.00251    0.00000    0.00000
AFIX  43
H1    2    0.000000    0.241437    0.180032    10.50000    0.67550
AFIX   0
PART 12
N2    4    0.079955    0.242691    0.044451    10.50000    0.08333    0.29000 =
         0.05261   -0.00544    0.02262    0.00049
HKLF 4




REM  triag2pbcl4_340a_a.res in Cmcm
REM wR2 = 0.0913, GooF = S = 1.151, Restrained GooF = 1.151 for all data
REM R1 = 0.0343 for 765 Fo > 4sig(Fo) and 0.0429 for all 905 data
REM 44 parameters refined using 0 restraints

END

WGHT      0.0383      7.7424

REM Highest difference peak  0.929,  deepest hole -2.164,  1-sigma level  0.200
Q1    1   0.4384  0.3531  0.2500  10.50000  0.05    0.93
;
_shelx_res_checksum              44794
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.24490(5) 0.250000 0.0262(6) Uani 1 4 d S T P . .
Cl2 Cl 0.500000 0.2447(4) 0.11861(14) 0.0657(12) Uani 1 2 d S T P . .
Cl1 Cl 0.7496(4) 0.4946(4) 0.250000 0.0851(14) Uani 1 2 d S T P . .
N1 N 0.1241(10) 0.2444(9) 0.1017(5) 0.076(3) Uani 1 1 d . . . . .
H1A H 0.222530 0.246236 0.114005 0.092 Uiso 0.5 1 calc R U P A 11
H1B H 0.222530 0.246236 0.114005 0.092 Uiso 0.5 1 calc R U P B 12
C2 C 0.080(2) 0.2427(17) 0.0445(6) 0.142(8) Uani 0.5 1 d . . P C 11
H2 H 0.147158 0.241656 0.010353 0.170 Uiso 0.5 1 calc R U P C 11
C1 C 0.000000 0.2431(16) 0.1374(7) 0.070(4) Uani 1 2 d S T P C .
H1 H 0.000000 0.241437 0.180032 0.7(9) Uiso 1 2 calc R . P . .
N2 N 0.080(2) 0.2427(17) 0.0445(6) 0.142(8) Uani 0.5 1 d . . P C 12
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0195(6) 0.0241(6) 0.0349(6) 0.000 0.000 0.000
Cl2 0.0344(15) 0.124(4) 0.0389(15) 0.0005(12) 0.000 0.000
Cl1 0.073(3) 0.075(3) 0.107(3) 0.000 0.000 -0.054(2)
N1 0.035(4) 0.112(9) 0.082(6) 0.004(4) -0.013(4) -0.004(3)
C2 0.083(9) 0.29(3) 0.053(6) -0.005(7) 0.023(6) 0.000(7)
C1 0.066(10) 0.090(12) 0.052(8) 0.003(5) 0.000 0.000
N2 0.083(9) 0.29(3) 0.053(6) -0.005(7) 0.023(6) 0.000(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 -8 1 0.0869
7 8 0 0.0832
1 11 -1 0.0738
-12 1 -1 0.4117
0 -11 1 0.0824
12 -1 -2 0.1383
1 0 -31 0.0656
0 0 31 0.0459
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Pb1 Cl2 179.94(12) . 10_556 ?
Cl1 Pb1 Cl2 90.02(4) 3_655 10_556 ?
Cl1 Pb1 Cl2 90.02(4) 3_655 . ?
Cl1 Pb1 Cl2 90.02(4) . . ?
Cl1 Pb1 Cl2 90.02(4) . 10_556 ?
Cl1 Pb1 Cl2 89.98(4) 5_445 10_556 ?
Cl1 Pb1 Cl2 89.98(4) 5_445 . ?
Cl1 Pb1 Cl2 89.98(4) 7_645 . ?
Cl1 Pb1 Cl2 89.98(4) 7_645 10_556 ?
Cl1 Pb1 Cl1 179.97(15) 3_655 7_645 ?
Cl1 Pb1 Cl1 179.97(15) . 5_445 ?
Cl1 Pb1 Cl1 84.169(16) 3_655 5_445 ?
Cl1 Pb1 Cl1 84.169(15) . 7_645 ?
Cl1 Pb1 Cl1 95.86(15) 5_445 7_645 ?
Cl1 Pb1 Cl1 95.80(15) 3_655 . ?
Pb1 Cl1 Pb1 179.97(15) . 5 ?
C2 N1 H1A 124.6 . . ?
C1 N1 H1A 124.6 . . ?
C1 N1 H1B 124.6 . . ?
C1 N1 C2 110.8(11) . . ?
C1 N1 N2 110.8(11) . . ?
N2 N1 H1B 124.6 . . ?
N1 C2 C2 106.3(8) . 12 ?
N1 C2 H2 126.8 . . ?
C2 C2 H2 126.8 12 . ?
N1 C1 N1 105.7(14) . 12 ?
N1 C1 H1 127.2 . . ?
N1 C1 H1 127.2 12 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Cl2 2.868(3) 10_556 ?
Pb1 Cl2 2.868(3) . ?
Pb1 Cl1 2.790(2) 3_655 ?
Pb1 Cl1 2.790(2) . ?
Pb1 Cl1 2.799(2) 5_445 ?
Pb1 Cl1 2.799(2) 7_645 ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C2 1.302(17) . ?
N1 C1 1.292(13) . ?
N1 N2 1.302(17) . ?
C2 C2 1.33(3) 12 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 N1 -1.4(14) . . . 12 ?
C1 N1 C2 C2 0.9(9) . . . 12 ?
N2 N1 C1 N1 -1.4(14) . . . 12 ?
